HRID1709773

反应详情

EQUATION

反应方程式

HRID 1709773 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of 1.0 g of 5,6-dichloro-2-[[(4-methoxy-3-methyl-2-pyridyl)methyl]thio]benzimidazole in 150 ml of methylene chloride and 30 ml of methanol was treated with 0.5 g of potassium carbonate. 0.6 g of m-chloroperbenzoic acid was added thereto at -30° while stirring, whereupon the solution was stirred for an additional 5 minutes and subsequently poured into a mixture of 20 ml of saturated sodium bicarbonate solution and 20 ml of water. The separated organic phase was dried over sodium sulfate, treated with 0.5 ml of triethylamine and evaporated in a vacuum. Crystallization from methylene chloride-methanol-ether yielded 5,6-dichloro-2-[[(4-methoxy-3-methyl-2-pyridyl)methyl]sulfinyl]benzimidazole of melting point 173°.

WORKUP

后处理

  1. stirringwas stirred for an additional 5 minutes
  2. dry with materialThe separated organic phase was dried over sodium sulfate
  3. additiontreated with 0.5 ml of triethylamine
  4. customevaporated in a vacuum
  5. customCrystallization from methylene chloride-methanol-ether